CN105118924A - Short-circuit-preventing top-emission OLED device and manufacturing method thereof - Google Patents
Short-circuit-preventing top-emission OLED device and manufacturing method thereof Download PDFInfo
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- CN105118924A CN105118924A CN201510453984.3A CN201510453984A CN105118924A CN 105118924 A CN105118924 A CN 105118924A CN 201510453984 A CN201510453984 A CN 201510453984A CN 105118924 A CN105118924 A CN 105118924A
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
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- H10K50/81—Anodes
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- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/17—Carrier injection layers
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- H—ELECTRICITY
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- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
- H10K2102/301—Details of OLEDs
- H10K2102/341—Short-circuit prevention
Abstract
The invention discloses a short-circuit-preventing top-emission OLED device and a manufacturing method thereof. Specifically, the OLED device comprises a substrate, a short-circuit-preventing reflective anode, a hole-injection layer, a hole-transporting layer, a light emitting layer, an electronic transmission layer also serving as a spacing layer, an electronic injection layer and a semi-transparent cathode. The manufacturing method comprises the following steps of (1) preprocessing the substrate; (2) performing vapor plating on an aluminum layer in the anode; (3) performing vapor plating on a silver layer in the anode; (4) performing vapor plating on the hole-injection layer; (5) performing vapor plating on the hole-transporting layer; (6) performing vapor plating on the light emitting layer; (7) performing vapor plating on the electronic transmission layer; (8) performing vapor plating on the electronic injection layer; (9) and performing vapor plating on the cathode. The device which adopts an aluminum/silver composite anode makes the high reflectivity characteristics of silver fully developed and meanwhile has the advantage of silver overcoming a device short circuit problem. The short-circuit problem of a pure silver anode is thoroughly solved. Meanwhile, the cathode thickness is optimized. Good conductive capabilities and relatively high light transmittance are further kept.
Description
Technical field
The invention belongs to microelectronics technology, be specifically related to top emission OLED device of a kind of against short-circuit and preparation method thereof.
Background technology
Organic Light Emitting Diode (OrganicLight-EmittingDiode, OLED) is the luminescent device of new generation of great potential, in flat panel display technology, large area light emitting illumination etc., have boundless application.It has self-luminous, all solid state, wide viewing angle, fast-response, anti-low temperature, can realize the characteristic such as low-voltage driving and Flexible Displays, demonstrates extremely strong competitiveness and development potentiality.
In display application, active-matrix Organic Light Emitting Diode (AMOLED) is main development trend, and its driving is controlled by thin-film transistor.If adopt the form of traditional bottom emitting, then when light is from substrate outgoing, inevitable by the electric circuit metal wire in glass substrate and TFT block, thus affect its aperture opening ratio.At present, no matter be the OLED display coordinating colored filter based on white OLED (WOLED), or based on the OLED display of RGB Organic Light Emitting Diode (RGBOLED), major part manufacturer all tends to the OLED form adopting top emitting, make its aperture opening ratio can reach 100% in theory, and then improve device lifetime and energy utilization rate.
Top radiation organic EL part is by transparent or translucent top cathode luminescence, and anode then adopts the metal material of high reflectance as reflector, and it can be produced on arbitrary substrate.Certainly can also adopt inverted structure, thus reach Seamless integration-with traditional amorphous silicon film transistor (a-SiTFT) N-shaped channel CMOS technique.
In existing industrialized producing technology, bottom anode generally adopts ITO/Ag/ITO structure.On the one hand, sputtering transparent indium-tin-oxide (ITO) and photoetching twice processing step bring great complexity to whole processing procedure; On the other hand, sputtering ITO indium used is more rare and valuable element, causes production cost to increase.In addition, if top cathode also adopts high-octane sputtering ITO, also damage can be brought to organic layer.Therefore, how simplification of flowsheet, avoids using high-octane ITO to sputter, and is the direction that everybody makes great efforts to explore.
At visible light wave range, the luminance factor aluminium of silver is eager to excel, and its conductance is the strongest in metal, and relative to aluminium, it is oxidized sex change not easily.As the anode of OLED, its work function is slightly larger than aluminium, is therefore more satisfactory anode material.But because the infiltration of silver to glass substrate is poor, when causing it to evaporate on a glass substrate as anode material, roughness is too large.Device operationally easily causes point discharge, thus causes short circuit.In OLED preparation, general sputtering silicon dioxide is as the resilient coating in glass substrate, and this adds the complexity of processing procedure undoubtedly.How effectively to play the strong point of silver and to simplify processing procedure simultaneously, be also this area problem demanding prompt solution.
Summary of the invention
For the problems referred to above, the invention provides a kind of top emission OLED device of against short-circuit, it comprises substrate and over the substrate by the anode at bottom to top successively evaporation, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer (doubling as wall), electron injecting layer and negative electrode, it is characterized in that:
Described anode is for having double-deck aluminium/silver-colored composite anode, wherein aluminium lamination is between described substrate and silver layer, the thickness of described aluminium lamination is 50 ~ 60nm and obtains through evaporation with the evaporation rate of 0.3 ~ 0.5nm/s, and the thickness of described silver layer is 40 ~ 50nm and obtains through evaporation with the evaporation rate of 0.2 ~ 0.3nm/s;
The thickness of described hole injection layer is 5 ~ 15nm;
The thickness of described hole transmission layer is 35 ~ 45nm;
The thickness of described luminescent layer is 15 ~ 25nm;
The thickness of described electron transfer layer is 10 ~ 15nm;
The thickness of described electron injecting layer is 10 ~ 20nm;
Described negative electrode is translucent fine silver negative electrode, and its thickness is 15 ~ 25nm.
Preferably, in technique scheme, any backing material that described substrate can select this area conventional, such as silicon chip, silicon dioxide, glass etc., preferred silicon chip or glass, more preferably glass.
Preferably, in technique scheme, the thickness of the aluminium lamination in described anode is 56nm, and the thickness of silver layer is 44nm.
Preferably, in technique scheme, the material of described hole injection layer is rare-earth oxide or organic material; Described rare-earth oxide is selected from molybdenum oxide (MoO
3), rheium oxide (ReO
3), tungsten oxide (WO
3) in any one, preferential oxidation molybdenum; Described organic material is selected from poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) (PEDOT:PSS), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine (m-MTDATA), 4,4', any one in 4''-tri-[N-(naphthalene-2-base)-N-phenyl amino] triphenylamine (2-TNATA), preferred PEDOT:PSS(structure is as follows); The thickness of described hole injection layer is 10nm.
Preferably, in technique scheme, the material of described hole transmission layer is selected from N, N'-diphenyl-N, N'-bis-(naphthalene-1-base)-1,1'-biphenyl-4,4'-diamines (NPB), N, N'-diphenyl-N, N'-bis-(3-aminomethyl phenyl)-1,1'-biphenyl-4,4'-diamines (TPD), 4, any one in 4'-bis-(carbazole-9-base) biphenyl (CBP), preferred NPB(structure is as follows); The thickness of described hole transmission layer is 40nm.
Preferably, in technique scheme, the material of described luminescent layer is three (oxine) aluminium (Alq
3) or the admixture (Alq of itself and (E)-4-dicyano methylene-2-tert-butyl group-6-[2-(l, l, 7,7-tetramethyl julolidine-9-base) vinyl]-4H-pyrans (DCJTB)
3: DCJTB), preferred Alq
3(structure is as follows); The thickness of described luminescent layer is 20nm.
Preferably, in technique scheme, the material of described electron transfer layer is selected from 4,7-diphenyl-1,10-phenanthroline (BPhen), 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBi), two (2-methyl-oxine-N1, O8) any one-(1,1'-biphenyl-4-hydroxyl) in aluminium (BAlq), preferred BPhen(structure is as follows); The thickness of described wall is 10nm.
Preferably, in technique scheme, the material of described electron injecting layer is the material of described electron transfer layer and the admixture of lithium, the preferably admixture (BPhen:Li) of 4,7-diphenyl-1,10-phenanthrolines and lithium, wherein the mass concentration of lithium is 2% ~ 3%, preferably 2.5%; The thickness of described electron injecting layer is 15nm.
Preferably, in technique scheme, the thickness of described negative electrode is 20nm.
On the other hand, present invention also offers a kind of method of the top emission OLED device for the preparation of above-mentioned against short-circuit, the method comprises the following steps:
1) preliminary treatment of substrate: substrate is cleaned in acetone, absolute ethyl alcohol and deionized water for ultrasonic successively and dries;
2) evaporation of the aluminium lamination in anode: use aluminium block to carry out evaporation on substrate described in step 1), controlling its evaporation rate is 0.3 ~ 0.5nm/s, until reach required thickness;
3) evaporation of the silver layer in anode: use Argent grain in step 2) described in aluminium lamination carries out evaporation, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
4) evaporation of hole injection layer: use hole injection layer material to carry out evaporation on silver layer described in step 3), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
5) evaporation of hole transmission layer: use hole transport layer material to carry out evaporation on hole injection layer described in step 4), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
6) evaporation of luminescent layer: use emitting layer material to carry out evaporation on hole transmission layer described in step 5), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
7) evaporation of electron transfer layer: use electron transport layer materials to carry out evaporation on luminescent layer described in step 6), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
8) evaporation of electron injecting layer: the mode being used as the electron transport layer materials of fertile material and dopant material to adulterate carries out common steaming on electron transfer layer described in step 7), the evaporation rate controlling described electron transport layer materials is 0.2 ~ 0.3nm/s, regulate its evaporation rate according to the doping ratio of described dopant material simultaneously, until reach required thickness, wherein said dopant material is lithium nitride, and the lithium discharged after its thermal decomposition is impregnated in described electron transport layer materials;
9) evaporation of negative electrode: use Argent grain to carry out evaporation on electron injecting layer described in step 8), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness, obtains the top emission OLED device of against short-circuit.
Preferably, in technique scheme, the time of ultrasonic cleaning described in step 1) is 5 ~ 20 minutes, preferably 10 minutes, and those skilled in the art have the ability to adjust concrete scavenging period according to selected substrate.
Preferably, in technique scheme, the temperature of drying described in step 1) is 110 ~ 150 DEG C, preferably 120 DEG C; Time is 10 ~ 30 minutes, preferably 20 minutes.
Preferably, in technique scheme, described evaporation has been come by the vacuum thermal evaporation instrument of routine.
Preferably, in technique scheme, for described evaporation various materials as defined above, and its purity is more than 99%; Wherein step 2) described in the diameter of aluminium block be 2 ~ 3mm; Described in step 3) and step 9), the diameter of Argent grain is 1mm.
Preferably, in technique scheme, after the top emission OLED device obtaining described against short-circuit, encapsulated, to reduce the destruction of oxygen and water vapour.
Compared with prior art, the tool of the present invention of technique scheme is adopted to have the following advantages:
(1) OLED of the present invention adopts aluminium/silver-colored composite anode, give full play to silver-colored high reflectance characteristic, taken into account aluminium as the advantage that can not cause shorted devices during anode simultaneously, and the optimum thickness of successful optimization composite anode (silver of the aluminium+44nm of 56nm), thoroughly solves the problem of fine silver as shorted devices during anode;
(2) aluminium of the present invention/silver-colored composite anode avoids the preparation process of sputtering ITO, simplifies preparation process; Avoid using storage rareness, expensive phosphide material simultaneously, greatly save cost of material;
(3) as the crystallization guide layer of silver, first aluminium be deposited in general substrate, and then stacked silver and form composite anode, thoroughly solves the problem of silver and the wettability difference of substrate, thus be conducive to overcoming shorted devices;
(4) thickness of the fine silver negative electrode in OLED of the present invention have also been obtained optimization: too thin then conductivity is lower, and too thick then light transmittance is poor; The thickness of about 20nm negative electrode is taken into account good conductive capability and larger light transmittance; In addition, employing evaporation silver electrode also avoid the damage that high-energy sputtering ITO is brought organic layer;
(5) top emitting device of the present invention is loose to the selection and comparison of substrate, is applicable to various backing material, compatible better;
(6) be conducive to using the Bphen of elements doped lithium as electron injecting layer reducing electron injection potential barrier and improving conductive capability; Simultaneously do wall as the Bphen of electron transfer layer is also double, be conducive to reducing to be diffused into due to lithium atom the fluorescence quenching caused in luminescent layer.
Accompanying drawing explanation
Fig. 1 is the curve chart of reflectivity along with wavelength change of fine aluminium anode and aluminium/silver-colored composite anode.
Fig. 2 is the reflectance curve figure that fixing aluminium/silver-colored composite anode gross thickness changes silver thickness.
Fig. 3 is the shape characteristic figure of the different metal film observed under AFM, and wherein (a) represents pure aluminium film (100nm), and (b) represents aluminium/silver composite membrane (56+44nm), and (c) represents fine silver film (100nm).
Fig. 4 is the layer structure schematic diagram of two kinds of top emission OLED device with different anode, and wherein (a) representative comprises the device of fine aluminium anode (100nm), and (b) representative comprises the device of aluminium/silver-colored composite anode (56+44nm).
Fig. 5 is the curve chart of luminous intensity with current density change of two kinds of top emission OLED device with different anode, and wherein (a) representative comprises the device of fine aluminium anode (100nm), and (b) representative comprises the device of aluminium/silver-colored composite anode (56+44nm).
Fig. 6 adopts fine aluminium electrode and the voltage-current density characteristic of aluminium/silver electrode composite as the OLED of anode and the performance chart of luminance-current density.
Fig. 7 adopts fine aluminium electrode and the current efficiency-current density of aluminium/silver electrode composite as the OLED of anode and the performance chart of optical power efficiency-current density.
Embodiment
Below with reference to the drawings and specific embodiments, the present invention is described in detail, but one skilled in the art will appreciate that protection scope of the present invention is not limited thereto.
Embodiment 1: the preparation of the top emission OLED device of against short-circuit.
About being described as follows of experiment material and instrument:
(background vacuum reading is lower than 4 × 10 to use conventional vacuum thermal evaporation instrument
-6torr) carry out evaporation, whole device is prepared and obtains in same cavity under continual vacuum condition; Draw-in groove substrate being placed on the rotating disk of the uniform rotation (about 30RPM) that gear motor drives deposits evaporated material to form resulting devices successively in the mode of being inverted (evaporation source under, substrate is upper); Organic layer and metal electrode layer carry out evaporation respectively by replacing mask plate; Use quartz-crystal Vibration Meter (SI-TM606A) Thickness Monitoring degree; Use the vapor-deposited film thickness that measurement of elliptically polarized li instrument (Alpha-SESpectroscopicEllipsometer) calibration is actual.
Concrete operation step is as follows:
(1) preliminary treatment of substrate: using (effective area is 0.09cm as the common optical glass of substrate
2, i.e. 0.3cm × 0.3cm) and clean 10 minutes in acetone, absolute ethyl alcohol and deionized water for ultrasonic successively, dry 20 minutes for 120 DEG C;
(2) evaporation of the aluminium lamination in anode: (diameter is about 5 ~ 6mm by high-purity little aluminium block, purchased from alfa, purity is 99.999%) cut into the square fritter of about 2 ~ 3mm, put into boron nitride crucible, evaporate with tantalum skin, adjustment current flow heats power, controlling its evaporation rate is 0.3 ~ 0.5nm/s, until the aluminium lamination of evaporation reaches 56nm on a glass substrate;
(3) evaporation of the silver layer in anode: use high purity silver particle (diameter is about 1mm, and purchased from alfa, purity is 99.99%), evaporate with tantalum skin, adjustment current flow heats power, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the silver layer of evaporation reaches 44nm on aluminium lamination;
(4) evaporation of hole injection layer: use high-purity MoO
3(light blue powder, purchased from alfa, purity is 99.998%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the hole injection layer of evaporation reaches 10nm on silver layer;
(5) evaporation of hole transmission layer: use high-purity N PB(pale yellow powder, purchased from alfa, purity is 98%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the hole transmission layer of evaporation reaches 40nm on hole injection layer;
(6) evaporation of luminescent layer: use high-purity Alq
3(yellow powder, purchased from alfa, 99%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the luminescent layer of evaporation reaches 20nm on hole transmission layer;
(7) evaporation of electron transfer layer: use high-purity BPhen(white powder, purchased from alfa, purity is 99%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the electron transfer layer of evaporation reaches 10nm on luminescent layer;
(8) evaporation of electron injecting layer: use high-purity BPhen(white powder, purchased from alfa, purity is 99%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, regulates dopant material lithium nitride (Li according to doping ratio simultaneously
3n) evaporation rate of (brown ceramic powder, purchased from alfa, purity is 99.4%, and the lithium discharged after thermal decomposition can be total to steaming and mix BPhen), until the electron injecting layer of evaporation reaches 15nm on the electron transport layer;
(9) evaporation of negative electrode: (diameter is about 1mm to use high purity silver particle, purchased from alfa, purity is 99.99%), evaporate with tantalum skin, adjustment current flow heats power, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the negative electrode of evaporation reaches 20nm on electron injecting layer, obtains the top emission OLED device of against short-circuit.
After the complete all material of evaporation makes device, in order to reduce oxygen and water vapour to the destruction of device, device adhering glass cover plate can be carried out simplified package.
Embodiment 2: the preparation of the top emission OLED device of against short-circuit.
Concrete operation step is as follows:
(1) preliminary treatment of substrate: using (effective area is 0.09cm as the common optical glass of substrate
2, i.e. 0.3cm × 0.3cm) and clean 5 minutes in acetone, absolute ethyl alcohol and deionized water for ultrasonic successively, dry 30 minutes for 110 DEG C;
(2) evaporation of the aluminium lamination in anode: (diameter is about 5 ~ 6mm by high-purity little aluminium block, purchased from alfa, purity is 99.999%) cut into the square fritter of about 2 ~ 3mm, put into boron nitride crucible, evaporate with tantalum skin, adjustment current flow heats power, controlling its evaporation rate is 0.3 ~ 0.5nm/s, until the aluminium lamination of evaporation reaches 60nm on a glass substrate;
(3) evaporation of the silver layer in anode: use high purity silver particle (diameter is about 1mm, and purchased from alfa, purity is 99.99%), evaporate with tantalum skin, adjustment current flow heats power, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the silver layer of evaporation reaches 50nm on aluminium lamination;
(4) evaporation of hole injection layer: use high-purity MoO
3(light blue powder, purchased from alfa, purity is 99.998%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the hole injection layer of evaporation reaches 15nm on silver layer;
(5) evaporation of hole transmission layer: use high-purity N PB(pale yellow powder, purchased from alfa, purity is 98%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the hole transmission layer of evaporation reaches 45nm on hole injection layer;
(6) evaporation of luminescent layer: use high-purity Alq
3(yellow powder, purchased from alfa, 99%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the luminescent layer of evaporation reaches 25nm on hole transmission layer;
(7) evaporation of electron transfer layer: use high-purity BPhen(white powder, purchased from alfa, purity is 99%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the electron transfer layer of evaporation reaches 15nm on luminescent layer;
(8) evaporation of electron injecting layer: use high-purity BPhen(white powder, purchased from alfa, purity is 99%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, regulates dopant material lithium nitride (Li according to doping ratio simultaneously
3n) evaporation rate of (brown ceramic powder, purchased from alfa, purity is 99.4%, and the lithium discharged after thermal decomposition can be total to steaming and mix BPhen), until the electron injecting layer of evaporation reaches 20nm on the electron transport layer;
(9) evaporation of negative electrode: (diameter is about 1mm to use high purity silver particle, purchased from alfa, purity is 99.99%), evaporate with tantalum skin, adjustment current flow heats power, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the negative electrode of evaporation reaches 25nm on electron injecting layer, obtains the top emission OLED device of against short-circuit.
After the complete all material of evaporation makes device, in order to reduce oxygen and water vapour to the destruction of device, device adhering glass cover plate can be carried out simplified package.
Embodiment 3: the preparation of the top emission OLED device of against short-circuit.
Concrete operation step is as follows:
(1) preliminary treatment of substrate: using (effective area is 0.09cm as the common optical glass of substrate
2, i.e. 0.3cm × 0.3cm) and clean 20 minutes in acetone, absolute ethyl alcohol and deionized water for ultrasonic successively, dry 10 minutes for 150 DEG C;
(2) evaporation of the aluminium lamination in anode: (diameter is about 5 ~ 6mm by high-purity little aluminium block, purchased from alfa, purity is 99.999%) cut into the square fritter of about 2 ~ 3mm, put into boron nitride crucible, evaporate with tantalum skin, adjustment current flow heats power, controlling its evaporation rate is 0.3 ~ 0.5nm/s, until the aluminium lamination of evaporation reaches 50nm on a glass substrate;
(3) evaporation of the silver layer in anode: use high purity silver particle (diameter is about 1mm, and purchased from alfa, purity is 99.99%), evaporate with tantalum skin, adjustment current flow heats power, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the silver layer of evaporation reaches 40nm on aluminium lamination;
(4) evaporation of hole injection layer: use high-purity MoO
3(light blue powder, purchased from alfa, purity is 99.998%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the hole injection layer of evaporation reaches 5nm on silver layer;
(5) evaporation of hole transmission layer: use high-purity N PB(pale yellow powder, purchased from alfa, purity is 98%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the hole transmission layer of evaporation reaches 35nm on hole injection layer;
(6) evaporation of luminescent layer: use high-purity Alq
3(yellow powder, purchased from alfa, 99%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the luminescent layer of evaporation reaches 15nm on hole transmission layer;
(7) evaporation of electron transfer layer: use high-purity BPhen(white powder, purchased from alfa, purity is 99%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the electron transfer layer of evaporation reaches 10nm on luminescent layer;
(8) evaporation of electron injecting layer: use high-purity BPhen(white powder, purchased from alfa, purity is 99%), evaporate on tantalum skin with quartz boat, controlling its evaporation rate is 0.2 ~ 0.3nm/s, regulates dopant material lithium nitride (Li according to doping ratio simultaneously
3n) evaporation rate of (brown ceramic powder, purchased from alfa, purity is 99.4%, and the lithium discharged after thermal decomposition can be total to steaming and mix BPhen), until the electron injecting layer of evaporation reaches 10nm on the electron transport layer;
(9) evaporation of negative electrode: (diameter is about 1mm to use high purity silver particle, purchased from alfa, purity is 99.99%), evaporate with tantalum skin, adjustment current flow heats power, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until the negative electrode of evaporation reaches 15nm on electron injecting layer, obtains the top emission OLED device of against short-circuit.
After the complete all material of evaporation makes device, in order to reduce oxygen and water vapour to the destruction of device, device adhering glass cover plate can be carried out simplified package.
Embodiment 4: the calculating of anode reflectance.
Adopt aluminium (50nm)+silver (50nm) as anode reflector, prepare corresponding Alq3 green glow OLED.Find after testing, this device is without short circuit phenomenon.On this basis, the method for optical thin film design is adopted to carry out thickness optimization design.Write MATLAB simulated program, fixing gross thickness is 100nm, and the silver calculating the aluminium+44nm of 56nm is optimum thickness.Now, the reflectivity in the silver-colored face of composite anode is the emergent light wavelength of the Alq3OLED device of 528nm(bottom emitting at wavelength) condition under be 93%, also slightly larger than the reflectivity (92.5%) of fine silver anode, and much larger than the reflectivity (87%) of fine aluminium anode, its result is as shown in Figure 1 and 2.
Embodiment 5: the roughness test of film.
In order to further confirmatory experiment designs, the present invention has prepared different metal films, and carries out morphology observation checking by atomic force microscope (AFM), and its result as shown in Figure 3.Can find, the film forming of pure aluminium film is very smooth, and crystalline state is good, and r.m.s. roughness is 1.32nm; But the roughness of fine silver film is very large, and r.m.s. roughness is 11.9nm; The roughness of aluminium/silver composite membrane is greatly improved, and r.m.s. roughness is 3.57nm, thus can overcome the problem of shorted devices.
Embodiment 6: adopt aluminium/silver composite membrane and pure aluminium film to test as the performance comparison of the OLED (without short circuit phenomenon) of anode respectively.
In order to embodiment 1 in adopt the OLED of aluminium/silver-colored composite anode ((b) in corresponding diagram 4) to contrast, prepared the OLED ((a) in corresponding diagram 4) adopting pure aluminium film as anode, wherein MoO
3as hole injection layer material, NPB is used as hole transport layer material, and Alq3 is used as emitting layer material, and Bphen is used as electric transmission and electron injecting layer material, and the Bphen of elements doped lithium is used as material spacer layer, and translucent fine silver film is used as cathode material.Because the conductive capability of hole transport layer material NPB is much larger than electric transmission and electron injecting layer material Bphen, the method changing thickness of hole transport layer is therefore adopted to regulate light path.Through repeatedly testing, obtain the thickness of detector parameter after optimization, as shown in Figure 4, the refractive index of layers of material also illustrates in the lump.
Test in self-built EL photoelectric test system, system is made up of constant-current supply (Keithley2400), photometer (PR655) and control software design.Every test data of the OLED obtained through EL photoelectricity test is as shown in Fig. 5 ~ 7.
Can find from Fig. 5, adopt the luminous intensity of the device of aluminium/silver-colored composite anode apparently higher than the device adopting fine aluminium anode.
Can find from Fig. 6 and Fig. 7, compared with adopting the OLED of fine aluminium anode, adopt the current efficiency of the OLED of aluminium/silver-colored composite anode to add 15%, optical power efficiency adds 25%.At 40mA/cm
2drive current density under, driving voltage drops to 4.6V from 5.2V.Under identical drive current density, adopt the luminosity of the device of aluminium/silver-colored composite anode higher than the device adopting fine aluminium anode.The above results all confirms, the top emission OLED device of the against short-circuit in the present invention has excellent photoelectric properties, overcomes the problems of the prior art, has the prospect of Depth Study and exploitation.
Claims (10)
1. a top emission OLED device for against short-circuit, it comprises substrate and over the substrate by the anode at bottom to top successively evaporation, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, it is characterized in that:
Described anode is for having double-deck aluminium/silver-colored composite anode, wherein aluminium lamination is between described substrate and silver layer, the thickness of described aluminium lamination is 50 ~ 60nm and obtains through evaporation with the evaporation rate of 0.3 ~ 0.5nm/s, and the thickness of described silver layer is 40 ~ 50nm and obtains through evaporation with the evaporation rate of 0.2 ~ 0.3nm/s;
The thickness of described hole injection layer is 5 ~ 15nm;
The thickness of described hole transmission layer is 35 ~ 45nm;
The thickness of described luminescent layer is 15 ~ 25nm;
The thickness of described electron transfer layer is 10 ~ 15nm;
The thickness of described electron injecting layer is 10 ~ 20nm;
Described negative electrode is translucent fine silver negative electrode, and its thickness is 15 ~ 25nm.
2. the top emission OLED device of against short-circuit according to claim 1, is characterized in that:
The thickness of the aluminium lamination in described anode is 56nm, and the thickness of silver layer is 44nm;
The thickness of described hole injection layer is 10nm;
The thickness of described hole transmission layer is 40nm;
The thickness of described luminescent layer is 20nm;
The thickness of described electron transfer layer is 10nm;
The thickness of described electron injecting layer is 15nm;
The thickness of described negative electrode is 20nm.
3. the top emission OLED device of against short-circuit according to claim 1, is characterized in that:
Described substrate be selected from silicon chip, silicon dioxide, glass any one, preferred silicon chip or glass, more preferably glass.
4. the top emission OLED device of against short-circuit according to claim 1, is characterized in that:
The material of described hole injection layer is rare-earth oxide or organic material; Described rare-earth oxide be selected from molybdenum oxide, rheium oxide, tungsten oxide any one, preferential oxidation molybdenum; Described organic material is selected from poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine, 4,4', any one in 4''-tri-[N-(naphthalene-2-base)-N-phenyl amino] triphenylamine, preferably poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid).
5. the top emission OLED device of against short-circuit according to claim 1, is characterized in that:
The material of described hole transmission layer is selected from N, N'-diphenyl-N, N'-bis-(naphthalene-1-bases)-1,1'-biphenyl-4,4'-diamines, N, N'-diphenyl-N, N'-bis-(3-aminomethyl phenyl)-1,1'-biphenyl-4,4'-diamines, 4, any one in 4'-bis-(carbazole-9-base) biphenyl, preferred N, N'-diphenyl-N, N'-bis-(naphthalene-1-bases)-1,1'-biphenyl-4,4'-diamines.
6. the top emission OLED device of against short-circuit according to claim 1, is characterized in that:
The material of described luminescent layer is three (oxine) aluminium or itself and (E)-4-dicyano methylene-2-tert-butyl group-6-[2-(l, l, 7,7-tetramethyl julolidine-9-base) vinyl] admixture of-4H-pyrans, preferably three (oxine) aluminium.
7. the top emission OLED device of against short-circuit according to claim 1, is characterized in that:
The material of described electron transfer layer is selected from 4,7-diphenyl-1,10-phenanthroline, 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene, two (2-methyl-oxine-N1, O8)-(1,1'-biphenyl-4-hydroxyl) any one in aluminium, preferably 4,7-diphenyl-1,10-phenanthrolines.
8. the top emission OLED device of against short-circuit according to claim 1, is characterized in that:
The material of described electron injecting layer is the material of described electron transfer layer and the admixture of lithium, the preferably admixture of 4,7-diphenyl-1,10-phenanthrolines and lithium, and wherein the mass concentration of lithium is 2% ~ 3%, preferably 2.5%.
9., for the preparation of a method for the top emission OLED device of against short-circuit according to any one of claim 1 to 8, it comprises the following steps:
1) preliminary treatment of substrate: substrate is cleaned in acetone, absolute ethyl alcohol and deionized water for ultrasonic successively and dries;
2) evaporation of the aluminium lamination in anode: use aluminium block to carry out evaporation on substrate described in step 1), controlling its evaporation rate is 0.3 ~ 0.5nm/s, until reach required thickness;
3) evaporation of the silver layer in anode: use Argent grain in step 2) described in aluminium lamination carries out evaporation, controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
4) evaporation of hole injection layer: use hole injection layer material to carry out evaporation on silver layer described in step 3), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
5) evaporation of hole transmission layer: use hole transport layer material to carry out evaporation on hole injection layer described in step 4), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
6) evaporation of luminescent layer: use emitting layer material to carry out evaporation on hole transmission layer described in step 5), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
7) evaporation of electron transfer layer: use electron transport layer materials to carry out evaporation on luminescent layer described in step 6), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness;
8) evaporation of electron injecting layer: the mode being used as the electron transport layer materials of fertile material and dopant material to adulterate carries out common steaming on electron transfer layer described in step 7), the evaporation rate controlling described electron transport layer materials is 0.2 ~ 0.3nm/s, regulate its evaporation rate according to the doping ratio of described dopant material simultaneously, until reach required thickness, wherein said dopant material is lithium nitride, and the lithium discharged after its thermal decomposition is impregnated in described electron transport layer materials;
9) evaporation of negative electrode: use Argent grain to carry out evaporation on electron injecting layer described in step 8), controlling its evaporation rate is 0.2 ~ 0.3nm/s, until reach required thickness, obtains the top emission OLED device of against short-circuit.
10. method according to claim 9, is characterized in that:
The time of described ultrasonic cleaning is 5 ~ 20 minutes, preferably 10 minutes;
The temperature of described oven dry is 110 ~ 150 DEG C, preferably 120 DEG C; Time is 10 ~ 30 minutes, preferably 20 minutes;
Described evaporation has been come by vacuum thermal evaporation instrument;
Purity for the various materials of described evaporation is more than 99%, and the diameter of wherein said aluminium block is 2 ~ 3mm, and the diameter of described Argent grain is 1mm.
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